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US9670567B2 - Manufacturing method of making aluminum alloy semi-finished product with improved microporosity - Google Patents

Manufacturing method of making aluminum alloy semi-finished product with improved microporosity Download PDF

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US9670567B2
US9670567B2 US13/398,691 US201213398691A US9670567B2 US 9670567 B2 US9670567 B2 US 9670567B2 US 201213398691 A US201213398691 A US 201213398691A US 9670567 B2 US9670567 B2 US 9670567B2
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molten metal
semi
ultrasound
micropores
metal bath
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US20120237395A1 (en
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Philippe Jarry
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Constellium Issoire SAS
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D1/00—Treatment of fused masses in the ladle or the supply runners before casting
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B21/00—Obtaining aluminium
    • C22B21/06—Obtaining aluminium refining
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
    • C22B9/02—Refining by liquating, filtering, centrifuging, distilling, or supersonic wave action including acoustic waves
    • C22B9/026—Refining by liquating, filtering, centrifuging, distilling, or supersonic wave action including acoustic waves by acoustic waves, e.g. supersonic waves
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/04—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling
    • Y02P10/234—

Definitions

  • the invention relates to semi-finished products made of aluminum alloy manufactured by vertical direct chill semi-continuous casting such as rolling slabs and extrusion billets, more particularly, such semi-finished products, their manufacturing methods and use, designed in particular for aeronautical and aerospace engineering.
  • Aluminum alloy plates and thick sections are used in particular in the aeronautical and aerospace engineering industry. These products are obtained in general by a method including vertical semi-continuous casting of a semi-finished product, rolling slab or extrusion billet, optionally the homogenization, hot working by rolling or extrusion, solution heat treatment and quenching of an aluminum alloy.
  • the most frequently used alloys are alloys of series 2XXX, series 7XXX and certain alloys of series 8XXX containing lithium.
  • damage tolerance properties may be influenced in particular by the presence in thick products of non-metallic inclusions and microporosity.
  • Micropores appear during slab casting and are then partially or completely filled by the rolling process. It is therefore attempted to eliminate micropores greater than approximately 90 ⁇ m which prove particularly detrimental for damage tolerance.
  • U.S. Pat. No. 5,772,800 describes a method for obtaining plates of thickness greater than 50 mm characterized by a density of micropores of size greater than 80 ⁇ m of less than 0.025 micropores per cm2 and a microporosity volume for the slab of less than 0.005%, in which the hot rolling conditions and the reduction ratios are adapted according to the radius of the hot rolling cylinder.
  • This method requires special tools for hot rolling and in certain cases, depending on the tools available and the thicknesses sought after, it is not possible to attain the transformation conditions that would allow the porosities to be filled efficiently.
  • degassing of the molten metal makes it possible to decrease the quantity of micropores in particular by decreasing the hydrogen content.
  • the hydrogen content in the molten metal is measured, for example, using a probe of the TelegasTM or AlscanTM type, known to those skilled in the art.
  • Known methods for decreasing the hydrogen content are, for example, treatment in a degassing ladle using a rotor by introducing chlorine and/or argon.
  • the use of ultrasonic emissions to degas the molten metal is also known.
  • Patent application CH 669.795 describes, for example, the introduction of ultrasonic heads into a conveying trough from a furnace to a foundry so as to obtain degassing.
  • Patent application US2007/235159 describes apparatus and a method in which an ultrasonic vibration is used to degas the molten metal in the presence of a purge gas such as argon or nitrogen.
  • U.S. Pat. No. 4,546,059 describes a method for continuous casting of light-alloys wherein ultrasound treatment is carried out in a solidification device optionally in an area separated from the solidification front by a porous material. This method results simultaneously in the formation of a uniform sub-dendritic structure, lowering of hydrogen content and reduction of porosity. To position the ultrasound head in the solidification device is not convenient.
  • a first subject of the present invention was to provide a manufacturing method for an unwrought aluminum alloy semi-finished product such as a rolling slab or extrusion billet.
  • the method includes:
  • a second subject of the present invention was the provision of a facility for vertical direct chill semi-continuous casting including at least one furnace necessary for melting the metal and/or for keeping it at a given temperature and/or for operations for preparing the molten metal and adjusting the composition, at least one vessel designed to perform a treatment to remove impurities that are dissolved and/or in suspension in the molten metal, a device for solidifying the molten metal by vertical direct chill semi-continuous casting including at least one ingot mould, a bottom block, a device to move downwardly, at least one device for procuring the molten metal and a cooling system, these various furnaces, pots and solidification devices being connected to each other by troughs in which the molten metal can be transported, characterized in that said installation also includes at least one immersed device comprising at least one ultrasound transmitter positioned in a furnace and/or a vessel.
  • FIG. 1 Micrographs without chemical attack of the solidified, unhomogenized metal obtained after ultrasound treatment of various durations: FIG. 1 a: 0 min, FIG. 1 b: 2 min, FIG. 1 c: 6 min, FIG. 1 d: 14 min, FIG. 1 e: 29 min.
  • FIG. 2 Micrographs without chemical attack of the solidified, unhomogenized metal obtained after ultrasound treatment of various durations: FIG. 2 a: 0 min, FIG. 2 b: 2 min, FIG. 2 c: 6 min, FIG. 2 d: 14 min, FIG. 2 e: 29 min.
  • FIG. 3 Histogram of micropores dimensions after homogenization, obtained by X-ray tomography.
  • the present inventor noted that, surprisingly, ultrasound treatment carried out upstream of casting makes it possible to decrease the dimension of micropores in solidified metal even if the hydrogen content and the grain structure are not modified.
  • the present inventor did not observe any degassing effect related to the ultrasound treatment but rather, an effect on the dimension of the micropores.
  • the present inventor thinks that this effect could be related to the later nucleation of micropores during solidification because of the better wetting of the inclusions by the molten metal in the presence of ultrasounds and to the fragmentation of said inclusions by the ultrasound treatment.
  • an ultrasound treatment carried out very upstream from the solidification device several minutes or several tens of minutes before casting, and which may have no or virtually no influence on either cast grain structure or hydrogen content, nevertheless enables to decrease microporosity of the cast product.
  • an ultrasound treatment carried out in a solidification device.
  • the preparation of the molten metal bath i.e. the adjustment of the composition of the alloy can be carried out according to methods known by those skilled in the art in an appropriate furnace.
  • other elements not mentioned may be present with a maximum content of 0.05 wt. % as impurities or minor additions.
  • the present invention is particularly advantageous for alloys whose Mg content is at least 0.1% by weight and/or whose Li content is at least 0.1% by weight.
  • it is particularly difficult to obtain a low hydrogen content by means of conventional degassing processes and, in addition, because of their high oxidability, the inclusion content is generally high.
  • the present invention makes it possible to obtain a low density of micropores with a dimension greater than approximately 90 ⁇ m, even with a high hydrogen content.
  • the method of the invention can be simplified compared to prior art methods in that there is no degassing step, the hydrogen content of the molten metal bath during solidification being at least 0.15 ml/100 g, preferably at least 0.25 ml/100 g and preferably still at least 0.30 ml/100 g.
  • the method according to the invention is particularly advantageous for alloys chosen from among AA2014, AA2017, AA2024, AA2024A, AA2027, AA2139, AA2050, AA2195, AA2196, AA2296, AA2098, AA2198, AA2099, AA2199, AA2214, AA2219, AA2524, AA5019, AA5052, AA5083, AA5086, AA5154, AA5182, AA5186, AA5383, AA5754, AA5911 AA7010, AA7020, AA7040, AA7140, AA7050, AA7055, AA7056, AA7075, AA7449, AA7450, AA7475, AA7081, AA7085, AA7910, AA7975.
  • the liquid metal undergoes ultrasound treatment in a furnace and/or a vessel (or “ladle”) using an immersed device comprising at least one ultrasound transmitter.
  • a vessel or “ladle” is a non-porous container wherein the metal can stay for controlled duration which depends of its dimension, the vessel being located between the furnace and the solidification device and enabling a treatment such as filtering the molten metal through a filter medium in a “filtration ladle” or introducing into the bath a “treatment” gas which may be inert or reactive in a “degassing ladle”.
  • the treatment using the device comprising at least one ultrasound transmitter it is typically helpful and may be necessary for the treatment using the device comprising at least one ultrasound transmitter to be carried out in a part of the casting facility in which sufficient treatment time is possible, upstream of the solidification device and not in a transfer trough wherein the residence time is too small.
  • no treatment by means of a gas such as argon, chlorine or nitrogen is carried out simultaneously with the ultrasound treatment.
  • ultrasound treatment conditions generating acoustic streaming are preferably avoided.
  • Gas treatment and/or acoustic streaming generate movements of metal carrying the oxides formed on the surfaces into the molten metal which is detrimental to the quality of the molten metal and the dimension of the micropores.
  • the ultrasound transmitter is used preferably at a frequency ranging between 18 and 22 kHz.
  • the treatment time advisable and/or necessary to obtain the desired effect required on the microporosity depends particularly on the power of the ultrasound transmitter used and the amount of metal treated.
  • the ultrasound treatment of a mass unit is preferably carried out at a total ultrasound power P for a length of time t such that the energy P ⁇ t is at least equal to a minimum energy per mass unit E min .
  • a minimum amount of energy E min of 4 kJ/kg, preferably at least 10 kJ/kg, and preferably still at least 25 kJ/kg, could prove to be sufficient during the treatment of a quantity of 16 kg with no stirring of the molten metal.
  • the total power P is at least equal to 400 W and/or time t is at least equal to 60 s.
  • the ultrasound treatment is carried out during casting, i.e. during the continuous flow in the molten metal solidification device, via a treatment vessel (or “ladle”).
  • the vessel is advantageously dimensioned so that the average residence time of a mass unit is at least equal to t min .
  • treatment using a device comprising at least one ultrasound transmitter is carried out before casting in a furnace.
  • the molten metal is stirred by electromagnetic means so as to circulate within the volume excited by the ultrasound transmitter.
  • An induction furnace can provide advantageous electromagnetic stirring, the frequency of the current used in the induction furnace can be adjusted to obtained a desired stirring.
  • the molten metal bath is at a temperature at least equal to 690° C. and preferably at least 700° C. during the ultrasound treatment. The less viscous the molten metal, the more effective the ultrasound treatment.
  • the molten metal bath can advantageously be at a temperature at least equal to 740° C. and preferably at least 750° C. during the ultrasound treatment.
  • the transfer of the liquid metal bath so treated to the solidification device is carried out in at least one trough (or “chute”), indeed these various furnaces, vessels and solidification devices are connected to each other by troughs in which the molten metal can be transported.
  • the duration elapsing between the end of ultrasound treatment of the liquid metal bath and the introduction of the same liquid metal bath in the solidification device is at least a few minutes, typically at least three minutes, particularly when the ultrasound treatment is carried out in a vessel, or even at least a few tens of minutes, typically at least one hour, particularly when the ultrasound treatment is carried out in a furnace.
  • the method according to the present invention makes it possible, for a given hydrogen content in the molten metal, to decrease the density of large-size micropores, which is particularly advantageous for certain alloys, such as alloys containing at least 0.1% Mg and/or 0.1% Li, for which it is difficult to reduce the hydrogen content.
  • the dimension of a micropore is the maximum dimension of the smallest ellipsoid which contains the micropore.
  • the method according to the present invention may comprise any number of further and/or conventional steps for treating molten metal such as filtration and/or degassing; this treatment may involve filtering the molten metal through a filter medium in a “filtration ladle” or introducing a “treatment” gas which may be inert or reactive into the bath in a “degassing ladle”.
  • the method according to the present invention can advantageously be carried out in a facility for vertical direct chill semi-continuous casting including at least one furnace necessary for melting the metal and/or for keeping it at a given temperature and/or for operations for preparing the molten metal and adjusting the composition, at least one vessel designed to perform a treatment to remove impurities that are dissolved and/or in suspension in the molten metal, a device for solidifying the molten metal by vertical direct chill semi-continuous casting including at least one ingot mould, a bottom block, a device to move downwardly, at least one device for procuring the molten metal and a cooling system, these various furnaces, vessels and solidification devices being connected to each other by troughs in which the molten metal can be transported, characterized in that it also includes at least one immersed device comprising at least one ultrasound transmitter positioned in a furnace and/or a vessel.
  • the device including an ultrasound transmitter is positioned in an induction furnace.
  • the unwrought semi-finished products obtained by a method according to the present invention advantageously have at mid thickness, a density of micropores of size greater than 90 ⁇ m less than 50% and preferably less than 20% of the density of micropores of size greater than 90 ⁇ m obtained by an identical method but not including ultrasound treatment step (ii).
  • the semi-finished products obtained with the method according to the present invention are particularly advantageous because even when their hydrogen content is high, the density of large-size micropores is particularly low.
  • semi-finished products obtained with the method according to the present invention are particularly advantageous in a homogenized state because they also have in this state, for which an increase in the dimension of micropores is typically to be observed, a particularly low density of large-size micropores.
  • the homogenization treatment is thermal treatment of the unwrought semi-finished product resulting from casting, which is carried out before hot working, at high-temperature, typically at a temperature greater than 450° C., the temperature depending on the alloy in question.
  • micropores tend to coalesce and therefore the maximum volume of micropores tends to increase, and similarly their dimension tends to increase even though homogenization also encourages spheroidizing that is a reduction of the surface/volume ratio.
  • Homogenization makes it possible to improve the metallurgical properties of the products, and is therefore particularly advantageous for obtaining a homogenized product with a low large-diameter micropores density.
  • the semi-finished products obtained with the method according to the invention optionally in a homogenized state, and whose hydrogen content is greater than 0.15 ml/100 g, or even at least 0.25 ml/100 g or even still at least 0.30 ml/100 g have a density of micropores of size greater than 90 ⁇ m less than 10/mm 3 and preferably less than 5/mm 3 .
  • Semi-finished products obtained with the method according to the invention with a lithium content of at least 0.1% by weight and preferably at least 0.8% by weight are particularly advantageous.
  • the semi-finished products obtained with the method according to the invention are particularly useful for applications in which the damage tolerance and in particular the fatigue strength of the products are great.
  • the semi-finished products obtained with the method according to the invention are therefore used in particular for manufacturing by rolling plates designed for the aircraft industry to produce spars, ribs, upper and lower wing skins and for manufacturing by extrusion sections designed for the aircraft industry to produce stiffeners.
  • the semi-finished products obtained with the method according to the invention are used for the manufacture of products obtained with low work-hardening and/or insufficiently compressive work-hardening such as products for which the ratio between the thickness of the semi-finished product and the thickness of the product after work-hardening is less than 4 or preferably 3.5 or 3.
  • the semi-finished products obtained with the method according to the present invention are, then, advantageous for the manufacture of thick products, of which the thickness is at least 100 mm, or preferably at least 125 mm.
  • the molten metal was held at a temperature of 700+5° C. throughout the test.
  • the hydrogen content was measured using an AlscanTM apparatus, used always outside the periods of ultrasound treatment so as not to disturb the operation of the probe.
  • the surface of the molten metal was swept permanently by argon at a rate of 5 l/min. No degassing or stirring was carried out.
  • microporosity of the samples taken in the shape of solidified slugs at a speed representing that of a rolling slab or an extrusion billet was characterized by optical microscopy.
  • the micrographs are shown in FIGS. 1 a to 1 e and 2 a to 2 e.
  • micropores dimension of these samples was measured by X-ray tomography after 12 hours' homogenization at a temperature of 505° C., which makes it possible to calculate the volume fraction of microporosity and the density of pores of size greater than 90 ⁇ m, 210 ⁇ m or 420 ⁇ m. Homogenization has the effect of increasing the micropores dimension.
  • FIG. 1a-FIG. 0.394 0.129 19.1 2.9 0.17 2a 2
  • FIG. 1b-FIG. 0.287-0.348 2b 6 (4 + 2)
  • FIG. 1c-FIG. 0.341-0.348 0.145 22.8 3.1 0.13 2c 14 (8 + 4 + 2)
  • FIG. 1d-FIG. 0.327 0.019 4.5 0.3 0 2d 29 (15 + 8 + 4 + 2)
  • FIGS. 1 and 2 show that in a rough-cast state, a very clear effect is observed for a 6-minute treatment at 500 W whereas no effect is detected for a 2-minute treatment at 500 W. In a homogenized state, a very clear effect is observed for a 14-minute treatment at 500 W, for which a reduction of more than 75% of micropores of size greater than 90 ⁇ m is to be noted.

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US13/398,691 2011-02-18 2012-02-16 Manufacturing method of making aluminum alloy semi-finished product with improved microporosity Active 2036-03-14 US9670567B2 (en)

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US201161444274P 2011-02-18 2011-02-18
FR1100505A FR2971793B1 (fr) 2011-02-18 2011-02-18 Demi-produit en alliage d'aluminium a microporosite amelioree et procede de fabrication
FR1100505 2011-02-18
US13/398,691 US9670567B2 (en) 2011-02-18 2012-02-16 Manufacturing method of making aluminum alloy semi-finished product with improved microporosity

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EP (1) EP2675932B1 (ru)
JP (1) JP2014506837A (ru)
CN (1) CN103392020B (ru)
BR (1) BR112013020976B1 (ru)
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